US4144202A - Dielectric compositions comprising ethylene polymer stabilized against water treeing with epoxy containing organo silanes - Google Patents

Dielectric compositions comprising ethylene polymer stabilized against water treeing with epoxy containing organo silanes Download PDF

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Publication number
US4144202A
US4144202A US05/864,750 US86475077A US4144202A US 4144202 A US4144202 A US 4144202A US 86475077 A US86475077 A US 86475077A US 4144202 A US4144202 A US 4144202A
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United States
Prior art keywords
dielectric composition
ethylene
dielectric
aryloxy
composition
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US05/864,750
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Arnold C. Ashcraft
Robert J. Turbett
Timothy R. Burke
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Union Carbide Corp
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Union Carbide Corp
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Priority to US05/864,750 priority Critical patent/US4144202A/en
Priority to AU42813/78A priority patent/AU533615B2/en
Priority to CA318,388A priority patent/CA1096159A/fr
Priority to ZA787180A priority patent/ZA787180B/xx
Priority to DK579578A priority patent/DK579578A/da
Priority to NO784362A priority patent/NO784362L/no
Priority to AR274964A priority patent/AR217887A1/es
Priority to JP15938678A priority patent/JPS5565246A/ja
Priority to BR7808480A priority patent/BR7808480A/pt
Priority to EP78101851A priority patent/EP0003050A1/fr
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Publication of US4144202A publication Critical patent/US4144202A/en
Assigned to MORGAN GUARANTY TRUST COMPANY OF NEW YORK, AND MORGAN BANK ( DELAWARE ) AS COLLATERAL ( AGENTS ) SEE RECORD FOR THE REMAINING ASSIGNEES. reassignment MORGAN GUARANTY TRUST COMPANY OF NEW YORK, AND MORGAN BANK ( DELAWARE ) AS COLLATERAL ( AGENTS ) SEE RECORD FOR THE REMAINING ASSIGNEES. MORTGAGE (SEE DOCUMENT FOR DETAILS). Assignors: STP CORPORATION, A CORP. OF DE.,, UNION CARBIDE AGRICULTURAL PRODUCTS CO., INC., A CORP. OF PA.,, UNION CARBIDE CORPORATION, A CORP.,, UNION CARBIDE EUROPE S.A., A SWISS CORP.
Assigned to UNION CARBIDE CORPORATION, reassignment UNION CARBIDE CORPORATION, RELEASED BY SECURED PARTY (SEE DOCUMENT FOR DETAILS). Assignors: MORGAN BANK (DELAWARE) AS COLLATERAL AGENT
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
    • H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
    • H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
    • H01B3/44—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes vinyl resins; acrylic resins
    • H01B3/441—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes vinyl resins; acrylic resins from alkenes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/54—Silicon-containing compounds
    • C08K5/541—Silicon-containing compounds containing oxygen
    • C08K5/5435—Silicon-containing compounds containing oxygen containing oxygen in a ring

Definitions

  • This invention relates to inhibiting electrical breakdown by water treeing in dielectric materials which are based on ethylene polymers.
  • compositions based on polyolefins are well-known and they are used extensively as insulation materials for wire and cable.
  • insulation materials properties of the composition such as intrinsic electrical strength, corona resistance and resistance to treeing are important.
  • Intrinsic electrical breakdown is the catastrophic failure of a dielectric accompanied by arcing or discharge through an ionized channel in the dielectric.
  • the intrinsic dielectric strength is considered to be an inherent property of the dielectric material.
  • Corona is an electrical plasma resulting from the ionization of a gaseous dielectric in regions of high electrical field. Corona resistance is the ability of a dielectric to withstand the corrosive action of an electrical plasma in contact with it.
  • olefin base compositions When used as a high voltage power cable insulation, olefin base compositions undergo a prebreakdown phenomenon known as treeing. This type of damage progresses through a dielectric section under electrical stress so that, if visible, its path looks something like a tree. Treeing can occur and progress slowly by periodic partial discharge, it may occur slowly in the presence of moisture without any partial discharge, or it may occur rapidly as the result of an impulse voltage. Trees may form at sites of high electrical stress such as contaminants or voids in the body of the insulation or at irregularities at the insulation-semiconductive screen interface.
  • Water treeing is a deterioration of a solid dielectric material which is simultaneously exposed to moisture and an electric field. It is a significant factor in determining the useful life of buried high voltage power cables. Water trees initiate from sites of high electrical stress such as rough interfaces, protruding conductive points, voids, or imbedded contaminants but at a lower field than that required for electrical trees. In contrast to electrical trees, water trees are characterized by: (a) the presence of water is essential for their growth; (b) no partial discharge is normally detected during their growth; (c) they can grow for years before reaching a size where they may contribute to a breakdown; (d) although slow growing, they are initiated and grow in much lower electrical fields than those required for the development of electrical trees.
  • a crosslinking agent may function as a water treeing inhibitor.
  • dicumyl peroxide is used as the crosslinking agent in polyethylene, for example, the peroxide residue functions as a tree inhibitor for some time after curing.
  • these residues are eventually lost at the temperatures of cable service. Therefore, in order to be an effective water treeing inhibitor an additive must be such that it is retained in the olefin composition at the temperature of cable service.
  • dielectric compositions based on ethylene polymers and used as insulation materials in high voltage wire ad cable are protected from water treeing under long term use under high voltage conditions, if the composition contains as a water treeing inhibitor, one or more organo silanes.
  • An object of the present invention is to provide a process for employing dielectric materials as insulation in high voltage wire and cable while protecting such dielectric material against water treeing.
  • Another object of the present invention is to provide dielectric materials which are resistant to water treeing in high voltage wire and cable and which retain this resistance under the conditions of use of the wire and cable.
  • a further object of the present invention is to provide a high voltage wire and cable which is resistant to water treeing.
  • the dielectric composition of the present invention comprises, in weight ratio,
  • organo silane compounds which are also described below.
  • the ethylene polymers which are used in the compositions of the present invention are solid (at 25° C.) materials which may be homopolymers, or copolymers of ethylene.
  • the ethylene copolymers contain at least 30 weight percent of ethylene and up to about 70 weight percent of propylene, and/or up to about 50 weight percent of one or more other organic compounds which are interpolymerizable with ethylene.
  • These other compounds which are interpolymerizable with ethylene are preferably those which contain polymerizable unsaturation, such as is present in compounds containing an ethylene linkage, > C ⁇ C ⁇ .
  • interpolymerizable compounds may be hydrocarbon compounds such as, butene-1, pentene-1, isoprene, butadiene, bicycloheptene, bicycloheptadiene, and styrene, as well as vinyl compounds, such as, vinyl acetate and ethyl acrylate.
  • copolymers could thus include those containing > 0 to 70 weight percent of propylene and 30 to ⁇ 100 weight percent of ethylene; and > 0 to ⁇ 50 weight percent butene-1 or vinyl acetate and 50 to ⁇ 100 weight percent of ethylene; and > 0 to ⁇ 30 weight percent of propylene, > 0 to 20 weight percent of butene-1 and 50 to ⁇ 100 weight of ethylene.
  • Preferred copolymers are ethylene/ethyl acrylate, ethylene/propylene, ethylene/butene and the like.
  • polymer also included in the term polymer are blends of one polymer with one or more other polymers.
  • blends are polyethylene with polypropylene, low-density polyethylene with high-density polyethylene, and polyethylene with olefins copolymers such as these indicated above.
  • the low density ethylene copolymers with ⁇ -olefins may be made under low pressure conditions of about 150 to 300 psi with supported chromium oxide based catalysts that are modified with titanium and optionally, fluorine, as disclosed in U.S. Pat. Nos. 3,606,736 and 4,011,382. The disclosures of these patents are included herein by reference.
  • the ethylene polymers described herein have a density (ASTM 1505 test procedure with conditioning as in ASTM D-1248-72) of about 0.86 to 0.96 grams/cubic centimeter and a Melt Index (ASTM D-1238 at 44 psi test pressure) of about 0.1 to 10 decigrams per minute.
  • organo silane which is employed in the dielectric compositions of the present invention is selected from one or more compounds of the following formula: ##STR1##
  • A is an epoxy containing radical
  • Y is C 1 to C 8 alkylene
  • R 1 is C 1 to C 8 Alkyl, C 1 to C 8 alkoxy, C 1 to C 8 acyloxy, C 6 to C 18 aryloxy or substituted aryloxy, such as p-acetylphenoxy
  • R 2 and R 3 are independently selected from C 1 to C 8 alkoxy, C 1 to C 8 acyloxy, C 6 to C 18 aryl or substituted aryl, C 6 to C 18 aryloxy or substituted aryloxy
  • a is an integer of 0 or 1.
  • the preferred organo silanes are selected from one or more compounds of the following formulae: ##STR2## wherein the R's are independently selected from hydrogen or C 1 to C 4 alkyl; R 1 , R 2 , R 3 and Y are as defined above; b is an integer of 1 to 2; c is an integer of 0 to 2; and d is an integer of 1 to 8.
  • organo silanes are generally known in the art and are prepared by methods as set forth in U.S. Pat. Nos. 2,970,150 and 2,946,701, for example, which patents are incorporated herein by reference.
  • organo silane encompassed by formula II is: ##STR3## while an example of an organo silane encompassed by formula II is: ##STR4##
  • the dielectric compositions of the present invention may also include cross-linking agents where the dielectric composition is to be used as a vulcanized composition rather than as a thermoplastic composition, and it is to be chemically cross-linked.
  • These chemical vulcanizing, curing or cross-linking agents are well known to those in the art and include the organic peroxide type of cross-linking agents which are disclosed for example, in U.S. Pat. Nos. 2,826,570, 2,888,424, 2,916,481, 3,079,370 and 3,296,189, the disclosures in such patents being incorporated herein by reference.
  • the chemical cross-linking agents may be used individually or in combination with one another, and they are used in cross-linking effective amounts.
  • the preferred cross-linking agent is a di- ⁇ -cumyl peroxide.
  • the dielectric compositions of the present invention also advantageously include one or more suitable high temperature antioxidants for the ethylene polymer in such compositions.
  • the antioxidants include sterically hindered phenols or amines. Polymerized 2,2,4-trimethyl dihydroquinoline may also be used. These are used in conventional amounts to obtain the intended effect in the composition.
  • the dielectric compositions of the present invention may also be extended, or filled, with polymers, other than the ethylene polymer, which are compatible, i.e., can be physically blended or alloyed, or grafted with the ethylene polymer.
  • the resulting compositions should contain at least about 30 weight percent of interpolymerized ethylene in all the polymers that may be present in the composition, based on the total weight of the resulting composition.
  • the other polymers which may be used would include polyvinyl chloride and polypropylene, ethylene propylene rubbers (EPR), ethylene, propylene, diene polymers (EPDM), styrene-butadienestyrene block copolymers, urethane elastomers, polyester elastomers, natural rubber.
  • EPR ethylene propylene rubbers
  • EPDM diene polymers
  • styrene-butadienestyrene block copolymers urethane elastomers
  • polyester elastomers natural rubber.
  • the total amount of adjuvants used will range from 0 to about 60 weight percent, preferably 0 to 10 weight percent based on the total weight of the dielectric composition.
  • All of the components of the dielectric compositions of the present invention are usually blended or compounded together prior to their introduction into the extrusion device from which they are to be extruded onto an electrical conductor.
  • the ethylene polymer and the other desired constituents may be blended together by any of the techniques used in the art to blend and compound thermoplastics to homogeneous masses.
  • the components may be fluxed on a variety of apparatus including multi-roll mills, screw mills, continuous mixers, compounding extruders and Banbury mixers.
  • compositions of the present invention are uniformly admixed and blended together, they are further processed, in accordance with the process of the present invention, in conventional extrusion apparatus at about 120° to 160° C. for crosslinkable compositions, and about 200° C. for thermoplastic compositions.
  • the crosslinkable compositions of the present invention are vulcanized at elevated temperatures of about 180° C. and preferably at 215°-230° C. using conventional vulcanizing procedures.
  • FIG. 1 shows a cross sectional view of the specimen where a is 152.4 millimeters, b is 24.4 millimeters and c is 19.05 millimeters.
  • the conical depression, W, of FIG. 1 is magnified in FIG.
  • d is 3.18 millimeters
  • e is 60 degrees
  • f is 3.18 millimeters
  • g is 6.35 millimeters
  • the tip radius is about 5 um.
  • the calculated maximum field is about 250 kV/mm in a typical 15 kV power cable.
  • each of the twelve conical depressions nearest the center of the specimen is punched out using a 12.7 millimeter (1/2 inch) circular die and an arbor press.
  • the resulting discs are placed in a boiling solution of 0.50 g methylene blue and 8 milliliter concentrated aqueous ammonia (28% approx.) in 250 milliliter distilled water for 30 minutes.
  • the discs are then sectioned and mounted on microscope slides for examination. Specimens prepared in this way have been kept for periods up to two years without apparent deterioration of the appearance of water trees.
  • FIG. 2 A typical water tree grown for 24 hours in low density polyethylene under the above conditions and stained as described, is depicted in FIG. 2.
  • the growth occurs in an approximately hemispherical region centered on the tip of the cone, which is usually heavily obscured. Because of this, the most satisfactory direction for measuring the extent of tree growth was found to be perpendicular to the side of the cone as indicated in FIG. 2. In our procedure all twelve of the stained trees from the central group of conical depressions are measured and the average length calculated.
  • L is the length of the growing tree and t is the time at which the measurement is taken, in hours.
  • Polyethylene homopolymer of 2.0 dg/min. Melt Index and 0.92 g/cc density, organo silane, antioxidant and dicumyl peroxide were charged to a Brabender mixer and compounded to a melt temperature no higher than 130° C.
  • the resulting composition was granulated and compression molded at 120° C., as heretofore described, and then cured in the mold at approximately 180° C.
  • the molded specimen was annealed in an oven at 115° C. for 15 minutes and then heated in a vacuum oven at 75° C. for 48 hours to remove byproducts of the peroxide decomposition.
  • the water tree growth rate was obtained by measuring the length of water trees formed in 24 hours and calculating the absolute rate of tree growth, as heretofore described by equations (1) to (7). A relative value of 1.0 for water tree growth rate was assigned to this composition.
  • WTGR Relative water tree growth rate
  • Example 1 was exactly repeated except that the composition was placed in a vacuum oven at 75° C. for 48 hours, after curing.
  • the WTGR for this composition was 0.82.
  • This Example shows that removal of peroxide residues, by treatment in a heated vacuum oven, reduces water treeing resistance as shown by the high value for WTGR.
  • Example 3 is exactly repeated except that the composition was placed in a vacuum oven at 75° C. for 48 hours.
  • the WTGR for this composition was 0.02.
  • This Example shows that heating under a vacuum does not reduce water treeing resistance when the composition contains an organo silane.
  • a crosslinkable composition containing polyethylene and such amounts and types of silane and amount of dicumyl peroxide, as set forth in the Table below were mixed according to Procedure B. Each composition also contained 0.15 percent each of thiodiethylene-bis(3,5- ditert butyl-4-hydroxy)-hydrocinnamate and distearyl-thiodiproprionate as antioxidants. After curing, each composition was placed in a vacuum oven at 75° C. for 48 hours. The WTGR was measured for each composition, and the results are as in the Table:

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  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
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US05/864,750 1977-12-27 1977-12-27 Dielectric compositions comprising ethylene polymer stabilized against water treeing with epoxy containing organo silanes Expired - Lifetime US4144202A (en)

Priority Applications (10)

Application Number Priority Date Filing Date Title
US05/864,750 US4144202A (en) 1977-12-27 1977-12-27 Dielectric compositions comprising ethylene polymer stabilized against water treeing with epoxy containing organo silanes
AU42813/78A AU533615B2 (en) 1977-12-27 1978-12-21 Dielectric polymer compositions
CA318,388A CA1096159A (fr) 1977-12-27 1978-12-21 Substances dielectriques protegees contre les arborescences par des composes a base d'organo-silane
ZA787180A ZA787180B (en) 1977-12-27 1978-12-21 Dielectric compositions stabilized against water treeing with organo silane compounds
NO784362A NO784362L (no) 1977-12-27 1978-12-22 Dielektrisk preparat.
DK579578A DK579578A (da) 1977-12-27 1978-12-22 Mod vandfremkaldt dendritisk gennemslag stabiliseret dielektrisk materiale
AR274964A AR217887A1 (es) 1977-12-27 1978-12-26 Composicion dielectrica y alambre o cable electrico
JP15938678A JPS5565246A (en) 1977-12-27 1978-12-26 Dielectric composition stabilized with organic silane compound against water treeing
BR7808480A BR7808480A (pt) 1977-12-27 1978-12-26 Composicao dieletrica e fio ou cabo eletrico
EP78101851A EP0003050A1 (fr) 1977-12-27 1978-12-27 Compositions diélectriques stabilisées contre le cheminement d'eau par des composés organosilanes, et câbles électriques isolés au moyen de ces compositions

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US05/864,750 US4144202A (en) 1977-12-27 1977-12-27 Dielectric compositions comprising ethylene polymer stabilized against water treeing with epoxy containing organo silanes

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EP (1) EP0003050A1 (fr)
JP (1) JPS5565246A (fr)
AR (1) AR217887A1 (fr)
AU (1) AU533615B2 (fr)
BR (1) BR7808480A (fr)
CA (1) CA1096159A (fr)
DK (1) DK579578A (fr)
NO (1) NO784362L (fr)
ZA (1) ZA787180B (fr)

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AR217887A1 (es) 1980-04-30
JPS575410B2 (fr) 1982-01-30
AU4281378A (en) 1979-07-05
EP0003050A1 (fr) 1979-07-25
AU533615B2 (en) 1983-12-01
JPS5565246A (en) 1980-05-16
ZA787180B (en) 1980-11-26
NO784362L (no) 1979-06-28
CA1096159A (fr) 1981-02-24
BR7808480A (pt) 1979-08-21
DK579578A (da) 1979-06-28

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Free format text: MORTGAGE;ASSIGNORS:UNION CARBIDE CORPORATION, A CORP.,;STP CORPORATION, A CORP. OF DE.,;UNION CARBIDE AGRICULTURAL PRODUCTS CO., INC., A CORP. OF PA.,;AND OTHERS;REEL/FRAME:004547/0001

Effective date: 19860106

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Owner name: UNION CARBIDE CORPORATION,

Free format text: RELEASED BY SECURED PARTY;ASSIGNOR:MORGAN BANK (DELAWARE) AS COLLATERAL AGENT;REEL/FRAME:004665/0131

Effective date: 19860925